反应详情

10.7 g (35.8 mmol) of 2,6-dimethyl-4-nitrophenyl trifluoromethanesulphonate (Example I) and 4.84 g (55.8 mmol) of LiBr are stirred in 120 ml of N-methylpyrrolidinone at 120° C. for 41 h. (Solvent: ethyl acetate/cyclohexane 1:4). After cooling, 80 ml of water are slowly added, and the mixture is stirred while cooling in an icebath for 1 h. The precipitate is filtered off with suction and stirred with 200 ml of petroleum ether. The solvent is removed in vacuo. 7.23 g (85%) of solid are obtained.

1. temperatureAfter cooling
2. temperaturewhile cooling in an icebath for 1 h
3. filtrationThe precipitate is filtered off with suction
4. stirringstirred with 200 ml of petroleum ether
5. customThe solvent is removed in vacuo